HPLC法测定盐酸美金刚多奈哌齐缓释胶囊中多奈哌齐的有关物质

Determination of the Related Substances in Memantine Hydrochloride and Donepezil Hydrochloride Extended-release Capsules by HPLC

目的:建立HPLC法测定盐酸美金刚多奈哌齐缓释胶囊中多奈哌齐的有关物质。方法:色谱柱:Inertsil ODS-SP C18(150 mm×4.6 mm,5μm),流动相:3.85 g·L-1的1-葵烷磺酸钠溶液-乙腈-高氯酸(650∶350∶1),流速:2.0 ml·min-1,检测波长:271 nm,进样体积:20μl,柱温:35℃。结果:盐酸多奈哌齐、杂质A、杂质B和杂质C定量限分别为0.2,0.1,0.2和0.2μg·ml-1,线性范围分别在0.40~6.05、0.20~3.02、0.20~2.99和0.20~3.04μg·ml-1内线性关系良好,相关系数r≥0.999 7;杂质A、杂质B和杂质C的平均回收率分别为99.82%,98.87%和100.64%,RSD分别为0.36%,0.23%和0.33%(n=9)。结论:该方法准确可靠,可用于盐酸美金刚多奈哌齐缓释胶囊中多奈哌齐的有关物质的测定。

Objective: To establish an HPLC method for the determination of the related substances in memantine hydrochloride and donepezil hydrochloride extended-release capsules. Methods: The column was Inertsil ODS-SP C18(150 mm×4.6 mm,5 μm),the mobile phase was buffer(3.85 g·L-1 sodium 1-decane sulfonate in water)-acetonitrile(650 ∶ 350) with 1.0 ml perchloric acid.The flow rate was 2.0 ml·min-1,the detection wavelength was 271 nm,the injection volume was 20 μl and the column temperature was 35℃ . Results: The quantification limit of donepezil hydrochloride,impurity A,impurity B and impurity C was 0.2,0.1,0.2 and 0.2 μg·ml-1,respectively. The linear relationship was good in the mass concentration range of 0.40-6.05,0.20-3.02,0.20-2.99 and 0.20-3.04 μg·ml-1,respectively,and the correlation coefficient r was ≥0.999 7. The average recovery of impurity A,impurity B and impurity C was 99.82%,98.87% and 100.64%,and the RSD was 0.36%,0.23% and 0.33%,respectively(n = 9). Conclusion: The method can be used for the determination of the related substances in donepezil hydrochloride of memantine hydrochloride and donepezil hydrochloride extended-release capsules.